Preparation of an alcohol-containing powder

ABSTRACT

Flowable powders having up to 60 percent ethyl alcohol content are prepared by the sorption of the alcohol with bulked, low dextrose equivalent dextrins. The resulting products are stable when hermetically packaged and are particularly qualified as alcoholic beverage forming compositions and flavoring materials.

United States Patent 1191 Mitchell et al.

[111 3,821,433 1*June 2a, 1974 1 PREPARATION OF AN ALCOHOL-CONTAINING POWDER [75] Inventors: William A. Mitchell, Lincoln Park,

N.J.; William C. Seidel, Monsey, NY.

[73] Assignee: General Foods Corporation, White Plains, NY.

The portion of the term of this patent subsequent to Mar. 19, 1991, has, been disclaim ed.

{22 Filed: Mar. 26, 1973 211 Appl. No.:345,143

Related US. Application Data [63] Continuation-impart of Ser. No. 240,272, March 31,

[ Notice:

[52] US. Cl 426/192, 426/213, 426/445, 426/471 [51] Int. Cl Cl2g 3/04 [58] Field of Search 99/28, 29, 30, 31, 78,

Primary Examiner-David M. Naff Attorney, Agent, or Firm-Howard .l. Newby; Bruno P, Strnzzi; Daniel J- Dkmovan [57] ABSTRACT Flowable powders having up to 60 percent ethyl alcohol content are prepared by the sorption of the alcohol with bulked, low dextrose equivalent dextrins. The resulting products are stable when hermetically packaged and are particularly qualified as alcoholic beverage forming compositions and flavoring materials.

4 Claims, No Drawings l PREPARATIONIOF 1 AN ALCOHOL-CONTAINING POWDER This application is a continuation-in-part of application Ser. No. 240,272, filed Mar. 31, 1972 for Alcohol- Containing Powder.

BACKGROUND OF THE INVENTION i; Field of thelnventio n The present invention generally relates to alcoholcontaining solids and, in particular, is directed to powders containing substantial amounts of alcohol. More specifically, the invention pertains to edible, ethanolcontaining carbohydrate powders.

2. Description of the Prior Art Prior efforts to make alcohol-containing edible powdered materials have been limited to the use of carbo-' hydrate materials in very dry conditionin order to have a significant amount of alcohol, specifically ethanol,

sorbed by the dehydrated solids. For the mostpar't, the prior arthas employed carbohydrates which are either 7 undesirably'sweet or those which dissolve with considbeverages havingtoo high viscosity, poor appearance and texture.

Sato, (Great'Britain Pat. No. 1,138,124) discloses the use of anhydrous lactose as a medium for'adsorping and/or absorbing ethanol. Sato identifies lactose. anhydride as the material for combination with the ethyl alcohol to provide a stable alcohol-containing powder and implies that anhydrous alcohol must be employed inthe preparation of the product since the presence of water would convert the lactose to theunacceptable hydrated crystalline form.

Bode, (US. Pat. No. 3,436,224) describes the preparation of an alcoholic dry beverage powder by dehydrating a vapor-sorbable particulated, starch based polysaccharide material to a moisture content of less than 0.75 percent and exposing the dehydrated material to anhydrous ethanol.

In both instances, it is to be noted, the prior art processes rely upon the substantially complete removal of physically or chemically. combined water from the solid prior to and during the sorption of ethanol by the dehy-' solutions.

SUMMARY OF THEINV'ENTION 7 Accordingly, it is an object of the present invention 4 to provide a flowable, high alcohol-containing powder which canbe produced in the presence of substantial quantities of moisture and which, when packaged in a sealed container, is stable. a

It is another object of the invention to provide a high ethanol-containing carbohydrate powder which readily dissolves in cold water to form a clear, low-viscosity, colorless liquid. i a

It is another object of the present invention to provide a high ethanol-containingpowder which is flowable and has a minimum tendency to lump and otherwise form compacted aggregates.

It isstill another object of the invention to provide a high ethanol-containing powder which can be used as a base for alcoholic beverages.

It is yet another object of the invention to provide a powder, which in addition to containing up to 60 percent ethyl alcohol is also amenable to the sorption of flavoring agents, particularly those usually employed in alcoholic beverages.

It is a feature of the invention that novel alcoholcontaining powders are produced by utilizing the heretofore unrealized capabilities ofcertain modified carbohydrates to sorb large quantities of ethanol when contacted and blended with the alcohol.

Briefly stated, the objects of the invention are accomplished by bulking, i.e., increasing the bulk volume and effective surface area of specific low D.E. (dextrose equivalent)dextrins and blending the bulked dextrins with liquid ethyl alcohol in ratios such that there is sufficient dextrin present to absorb/adsorb the available ethanol and produce a dry'-to-the-touch flowable powder incorporated with up to about 60 percent ethanol. When hermetically packaged, even though the alcohol containingpowders have, in addition to 60 percent alcohol by weight, as much as 4.6 percent water, they remain chemically stable and in flowable physical condition. The products of the invention can have excellent cold water solubilities and reconstitute to provide nonsweet, low viscosity, clear colorless and sparkling liquid solutions.

The essence of the invention resides in the discovery that dextrins having low dextrose equivalent values of from about 5 DE. to about 15 D.E. and which have been expanded to a low bulk densityof from about 0.05g/cc to about 0.30g/cc have the capability for adsorbing/absorbing large amounts of alcohol. Among these dextrins are some special dextrins which are excellentfilm-forming materials; which can be bulked (as above) to produce low bulked density materials whose bulked physical conditions are not easily altered upon compression; and which are distinguished from the normal dextrins by having the capabilities of dissolving readily in cold water to form clear, sparkling, low viscosity and non-sweet solutions with no off-flavors. Such special dextrins have a D.P. (degree of polymerization) of from 1 to about 20 glucose units with an average DR of about 10 (molecular weight about 1,600). Furthermore, in comparison with the normal dextrins, the special dextrins, which can be produced by enzymatic hydrolysis ('e.g., alpha amylase from B. Subtilis) contain about 10 percent less polymers in the DP. range about 10 than the normal dextrins having .the same DE. and they have a preponderance of trimer, hexamer and heptamer content equivalent to more than 50 percent of the oligomers (D.P. l0 and below). Additionally, the special dextrins have only a trace to about 1 percent glucose and a very limited amount of maltose. The preparation of the special dextrins is discussed hereinbelow.

in summary, the-low sweetness level of these special dextrins is derived from the limited amount of glucose and maltose present, the low viscosity and good solubility and clarity is due to the reduced level of the higher D.P. materials, and the lack of off-flavors results from the use of enzymes for their preparation in contrast to the conventional acid and/or heat dextrinization. These features of the special dextrins make them particularly DESCRlPTlON OF THE PREFERRED EMBODIMENTS The special dextrin substances preferred for the purposes of the present invention are prepared by special and proper alpha-amylase degradation such that maltose and dextrosev production are limited. Under these conditions, the DE. is allowed to reach 5 to or and the dextrins contain little glucose and an irregular distribution of polymeric members with a preponderance (greater than 50 percent) of trimer, hexamer and heptamer polymers of glucose in the oligosaccharide range.

Briefly, the special dextrins are prepared from corn starch, tapioca starch, potato starch and other starches by the modification of these starches by alpha amylase (B. Subtilis) in accordance with the general procedures described in texts on the subject such as Chemistry and Industry of Starch, Academic Press Inc., New

York, N.Y. 1950 edited by R. W. Kerr. lmportantly,

the dextrinization of the starch is conducted under carefully controlled conditions of time and temperature to effect a modification of the starch such that the resulting dextrose product, when analysed by standard analytical techniques, including chromotography analysis, has a DB. of 5 to 15 with little or no glucose and an irregular distribution of polymeric members with a preponderance (greater than 50 percent of trimer, hexamer and heptamer polymers of glucose in the oligosaccharide range. Although there can be small variations in the temperature range and thetime to effect proper conversion, depending primarily on the type and degree of purity of the starch, the procedure normally requires maintaining the starch in aqueous suspension with the enzymes for a period of to 39 minutes during which the temperature of the suspension is uniformly increased from room temperature to 65 75C. A detailed description of the dextrinization of a typical starch to produce a dextrin suitable for purposes of the invention is disclosed in Example l (below). Commercially, available corn syrup dextrins, typified by the products of C.P.C. lntemational, Englewood Cliffs, NJ. under the trade name MGR-REX, have a similar functionality for purposes of the instant invention as that described above and, upon analysis have been shown to have the irregular distribution of polymeric members with a substantially similar preponderance of trimer, hexamer and heptamer polymers of glucose in the 'oligosaccharide range with little or no glucose present.

The dextrins, as prepared, have a bulk density of approximately O.4O.6g/cc and, although they have some affinity for ethyl alcohol in this physical form, a significant increase in their capabilities for adsorbing/absorbing ethyl alcohol has been found to result when they are expanded such that their bulk densities are decreased to from about 0.05g/cc to about 0.30g/cc. The procedure for bulking (expanding) the dextrins to the extent of maximizing their effective surface areas to unit weight ratios is an important operation in the practice of the process according to the invention.

Although various bulking techniques including spray drying can be employed, the preferred method for physically expanding the dextrins to a high bulk volume for enhancing their capabilities to sorb ethyl alcohol comprises forming a very thin continuous film of a water solution of the dextrin followed by drum drying the film. The bulking method can best be accomplished by drying the dextrin film from about a percent aqueous solution of dextrin on an atmospheric d-rum dryer. The drum dryer roll surfaces are heated from within the drum chambers with steam at about psig and the rolls are rotated at a circumferential speed of about 15 20 ft. per minute. These preferred conditions, of course, can be modified the important criteria being that the dextrins should be uniformly blended with an amount of water sufficient to effect the formation of a continuous film during the drying step. The thin film of dextrin is dried to a moisture content of from about 2 percent to about 6 percent and, when doctored from the rolls forms fine particles of high bulk volume. Drum drying the dextrin material in this manner produces expanded, and not easily compressed, particles of low density, which are amorphous but crystalline-appearing materials, and which are nonhydroscopic and dissolve easily in water. After drying, the products can be comminuted and screened, if desired, to remove particles that are either too large or too fine. The most preferred particle size fraction for practicing the invention is that which passes through a 20 mesh screen and is held on a 60 mesh screen (U.S. Standard Sieve) and has a bulk density of from about 0.10 to about 0.15 per cubic centimeter.

because of their rapid and complete solubility in cold water to form water-white solutions with low viscosities. Specifically, the special dextrins are of a sufficient low average molecular weight to be readily soluble in cold water; they have excellent film-forming properties which permits them to be bulked and, are further characterized by their lack of off-flavor and sweetness.

The bulked 5, l0, and 15 D.E. special dextrins are products which exhibit rapid and complete solubility in cold water to form clear, colorless solutions. At a concentration of 40 percent by weight in aqueous solution, the 10 DE. dextrin has a viscosity of about centipoise at F.

The special dextrins have low moisture absorption relative to the normal dextrins above DE. The 10 D.E. dextrin at 70 percent relative humidity and 77F. absorbs up to about 13 percent moisture. While each of the bulked dextrins of the invention has excellent affinity for ethyl alcohol, the 5 DE. dextrin has the capability of sorbing more of the alcohol, especially when some water is present and, for this reason, is the preferred carbohydrate material for the purposes of the invention.

in contrast to the prior art it is not essential to the success of the invention that anhydrous alcohol be employed for sorption by the dextrin. Surprisingly, it has been found that aqueous alcohol solutions can be sorbed to form alcohol/water-containing stable, flow able powders. While alcohol with a minimum of associated water is preferred, (primarily from the viewpoint of the desirability of having a high concentration of alcohol in the powder), ethyl alcohol having as much as percent dissolved water can be sorbed by the bulked 5 DE. dextrin (0.16g/cc and 4.1 percent moisture) to form a stable,,flowable powder containing 32 percent ethyl alcohol, 10.5 percent water and 57.5 percent dextrin solids. If the bulked 5 DE. dextrin has a 1 2 percent moisture content more water can be included in theal'cohol solution to be sorbed. For example, a 5 D.E.dextrin at this initial low moisture content will sorb 40 percent by weight of an alcohol solution containing percent water and produce a product containing percent alcohol, 13 percent water and 57 percent dextrin solids. This is about the maximum amount of water that can be held by this dextrin. Alternatively, the bulked 5 DE. dextrin, when contacted with 95 percent by weight alcohol aqueous solution will sorb sufficient solution to form a flowable powder containing 60 percent alcohol, 35.4 percent dextrin and 4.6 percent water.

Each of the above dextrins can be combined with ethanol to form the products of the invention by sorption of the alcohol by the dextrin in the course of a blending procedure. The addition of appropriate quantities of the alcohol .to the dextrin, or vice versa, in a vessel followed by gentle, but thorough mixing, affords adequate inducement for adsorption/absorption to take place resulting in a flowable powder.

Once the alcohol-containing powdered product has been prepared it is stable for extended time periods provided it is hermetically packaged. Such packaging is necessary for stability because the product (as is the case with the prior art products) develops an ethanol vapor pressure greater than atmospheric pressure at room temperature. However, in a vapor-tight package, the product retains its alcoholic content, remains dryto-the-touch, and retains its original flowable'condition characterized by being pourable or spoonable from the container with little or no tendency to clump or otherwise aggregate. When produced for alcohol beverage purposes, each of the products can be readily tailored to contain either water soluble or ethyl alcohol soluble flavoring ingredients which are usually employed in mixed alcohol beverages. Alternatively, the products of is sufficiently high to ignite and support combustion and the products may be used as flaming agentsfor appropriate desserts. Also, the products of the invention find utility as powdered carriersifor alcohol soluble flavors which would normally be degraded or lost upon drying.

The following examples illustrate the various facets of the invention. It should be understood, however, that these examples are meant to be illustrative and the invention is not to be limited thereto. In the examples which follow, g stands for grams, cc stands for cubic centimeters, D.E." for dextrose equivalents, and the percentages provided are percentages by weight.

EXAMPLE I A 0.8g quantity of alpha amylase (B. Subtilis) (Takamine PIT-1,000) was dissolved in 800 ml of water. Four hundred grams of potato starch was then mixed into the enzyme solution and themixture placed in a C. water bath and stirred. In approximately 8 minutes the temperature of the aqueous mixture reached 65C. and the starch began to thicken (swell). As the temperature increased to 67C. the enzyme activity became apparent and the slurry became less viscous. After 21 minutes and at a temperature of 71C. the mixture was clear. The mixture was then quickly heated to the boiling point to deactivate the enzyme, then filtered, and boiling was then continued to concentrate the solution to a heavy syrup. The syrup was then vacuum dried.

The dried dextrin was determined by standard analytic technique to have a dextrose equivalent of 5, a glucose content below 1 percent, and a chromomatographic analysis showed an irregular distribution of the polymeric members with a preponderance (greater than 50 percent) of trimer, hexamer and heptamer polymers of glucose in the oligosaccharide range.

1 EXAMPLE II Approximately 400 g of the 5 DE. dextrin of Example l was added to 400 g of water to form a clear colorless solution. The solution was uniformly applied to the surfaces of heated drum dryer rolls. The solution formed a thin continuous film on the atmospheric drum dryer roll surfaces which were heated from within the roll chambers by steam at 60 psig. The 18 inch diameter rolls were rotated at 3 rpm and the dried solution of dextrin was then doctored from the rolls in the form of small particles having an average bulk density of 0.16g/cc and a moisture content of 5.5 percent.

EXAMPLE lll A 150g amount of the bulked 5 DE. dextrin of Example II was blended with 250g of percent (l0 percent by weight water) ethanol in a Hobart mixer at speed No.2 with a wire whisk for 2 minutes. A a dry-tothe-touch free flowing powder was obtained that contained 56.2 percent ethanol and 8.3 percent moisture. The bulked ethanol containing flowable powder was packaged in air-tight foil envelopes and after 6 months theinvention may be added to water with commercial cocktail mixes to form alcoholic beverages of excellent qualities.

In addition, the alcohol-containing powders disclosed herein can be marketed as ingredients in dry pudding and topping mixes. The alcohol content of the products storage had retained its fiowability characteristics and its original alcohol content.

EXAMPLE IV A teaspoonful (3g) of the product of Example lll when added to 10ml of water produced a clear, sparkling low-viscosity alcoholic solution with a non-sweet strong alcohol taste.

EXAMPLE V A 28g quantity of the product of Example III was blended withone package (17.7g) of Holland House Daiquiri Mix to 3 02s. of water and a small quantity of crushed ice and shaken vigorously. The resultant mixture produced a daiquiri beverage of excellent quality.

EXAMPLE VI The procedure described in Example I was modified only to the extent of extending the time of dextrinization to produce a DE. dextrin which was then bulked (Example II) to an average density of 0.15g/cc and a moisture content of 1.5 percent.

EXAMPLE VII EXAMPLE Vlll To 2.8g of freeze-dried coffee was added 8.5g of the expanded ethanol containing powder of Example "I to produce a flowable powdered mixture. A 175 ml of hot water was added to a heaping teaspoon of the mixed powders to produce a unique coffee beverage. The bev-, erage had excellent flavor and the alcohol content of the beverage appeared to enhance the coffee flavor notes.

EXAMPLE IX To 40g of the bulked dextrin of Example III were added 60g of 95 percent alcohol containing 500 of Firmenich liquid wine flavor (P.F.W.570039).'A uniform blend of a free flowing powder was obtained. This 'powv der was dissolved in 500 ml cold water and then 500 ml of cold club soda was added. A pleasant carbonated wine beverage was produced.

EXAMPLE x A liberal quantity of the alcohol-containing powder prepared as in Example III was sprinkled over a fruit cocktail serving. The presence of the alcohol enhanced the fresh fruit flavors of the fruit flavors of the fruit cocktail.

EXAMPLE Xl A liberal quantity of the alcohol-containing dextrin prepared in Example lll was sprinkled over a broiled steak and ignited. The material burned with a controlled blue flame and was then extinguished before excessive charring could take place.

By the foregoing, the present invention has been described in such detail as to enable others skilled-in-theart to make and use the same, and, by applying current knowledge, adopt the same for use under varying conditions of service, without departing from the essential features of novelty thereof, which are intended to be defined and secured by the appended claims.

What is claimed is:

l. A method of preparing a flowable, dry-to-thetouch, alcohol-containing powder which consists of:

a. dissolving in water a dextrin having a dextrose equivalent of from about 5 to about 15 and further characterized by having more than 50 percent of the trimer, hexamer and heptamer oligomers by weight of its total oligomer (10 or less degrees of polymerization) content and less than about 1 percent glucose,

b. expanding the dextrin by forming a film of the solution of (a) and drum drying said film,

v c. subdividing the dried film of dextrin to yield particulates of expanded dextrin having a size corresponding to a 20 mesh screen opening (U.S.S. Sieve), a moisture content ranging from about 2 percent to about 6 percent and a bulk density ranging from about 0.05 to about 0.30 grams/cubic centimeter, and

d. contacting the expanded dextrin of ('c) with an aqueous solution of ethanol so as to cause the dextrin to sorb from about 30 percent to about 60 percent ethanol by weight of the resulting flowable ethanol-containing powder.

2. An ethanol-containing flowable powder composition prepared by the method of claim 1.

3. The composition of claim 2 which further contains an effective amount of a food flavoring material.

4. The composition of claim 2 which further contains an effective amount of an alcoholic beverage flavoring 

2. An ethanol-containing flowable powder composition prepared by the method of claim
 1. 3. The composition of claim 2 which further contains an effective amount of a food flavoring material.
 4. The composition of claim 2 which further contains an effective amount of an alcoholic beverage flavoring material. 